CN1307338C - Neat oil finish with high lubricant content - Google Patents

Abstract

A lubricating finish composition and synthetic filaments coated with the composition. The composition of the invention comprises: about 80 to about 99 weight percent lubricant; and about 1 to about 20 weight percent sodium or potassium alkali metal salt of a branched or unbranched aliphatic monocarboxylic acid having at least 8 carbon atoms. The finish composition is a liquid at a temperature below about 150 DEG C.

Description

Lubricating finish composition, method of use thereof, and synthetic fibers coated therewith

This application is a divisional application of the invention patent application with the filing date of February 19, 1993 and the application number of 93103441.8.

The present invention relates to a finishing agent composition for synthetic fibers, more specifically a pure oily finishing agent composition and synthetic fibers coated with the composition.

Typical known neat oil finishes for polyamide and polyester yarns contain very high percentages of nonionic surfactants, eg 30% by weight. It provides yarn with good static charge removal, yarn bundle cohesion and ideal wetting properties. However, such high percentages of nonionic surfactants in the finish also present disadvantages in that they generally increase the viscosity of the finish, thereby making it difficult to apply the finish evenly. In addition, nonionic surfactants increase the degree to which finishes are subjected to oxidative degradation and produce fumes when heated. These disadvantages are even more pronounced when such finishes are used as "spin finishes" in the production of high strength polyamide and polyester industrial yarns using high draw ratios and high temperatures.

There can also be trouble when there are nonionic surfactants in neat oil finishes when using yarns in woven fibers. Nonionic surfactants are sometimes incompatible with sizing, especially polyacrylic acid sizing, and can cause sizing, weaving and laundering problems for fibermakers.

To improve the application uniformity of high viscosity pure oil finishes containing nonionic surfactants, low molecular weight diluents, such as mineral spirits, are sometimes added to reduce the viscosity of the finish. These diluents, however, increase the fuming properties of the finish, thereby posing fire and explosion hazards, as well as health and environmental concerns. Using higher finishing temperatures to reduce viscosity is also not ideal for finishes containing higher percentages of nonionic surfactants because doing so increases thermal degradation. If an attempt is made to reduce the content of non-ionic surfactants, in order to reduce their percentages, for example by 5% by weight of such surfactants, and to replace them with additional lubricants, the result will again be found in yarn manufacture and subsequent The antistatic performance of the finishing agent is reduced during the use of the finished product.

The invention provides a lubricating finishing agent composition and synthetic fibers coated with the composition. Compositions of the present invention include:

about 80-90% by weight of a lubricant; and about 1-20% by weight of an alkali metal salt of a branched or unbranched aliphatic monocarboxylic acid containing at least 8 carbon atoms. At temperatures below about 150°C, the finish composition is a liquid.

Preferred lubricants are those selected from the class consisting of natural and synthetic esters and natural and synthetic hydrocarbons having a number average molecular weight of at least about 550 atomic mass units (amu) and an iodine value of less than 15. In a preferred embodiment of the present invention, the finish composition is substantially free of nonionic surfactants, preferably branched or unbranched aliphatic-carboxylic acids having at least about 14 carbon atoms. Salt.

According to the invention, the lubricating finish is suitable for use as a pure oily finish for synthetic fibers including polyamide and polyester multifilament yarns, in particular as a "spin finish" for industrial yarns. The finishing agent of the present invention can provide electrostatic protection performance while avoiding the problem of high viscosity caused by the use of high percentage of nonionic surfactant. In addition, testing conducted in the hot coating test showed that preferred finish compositions containing optional stabilizers had much improved thermo-oxidative stability. The preferred finish compositions also exhibit low smoking properties. The finish composition is readily compatible with polyacrylic sizing when the yarn is used to weave fibers.

The finish compositions of the present invention comprise 80-99% by weight lubricant, preferably about 85-98% by weight. The lubricant should be a lubricant or a mixture of lubricants suitable for use in pure oily finishes and so as not to get on hot machine parts during spinning of the yarn or in subsequent use of the finished product Excessive smoke generation. Preferably, the lubricant is selected from the class consisting of natural and synthetic esters and natural and synthetic hydrocarbons having a number average molecular weight of at least about 550 amu.

The lubricant is liquid at or below room temperature to allow easy handling even at low temperatures and consistent end-use performance. For some finished applications, however, a solid lubricant that melts at or above room temperature may be more desirable. In any event, the melting point of the lubricant should not be too high since in order for the composition to be an effective pure oil finish it is necessary for the finish composition to be a liquid at temperatures below about 150°C. To prevent oxidative degradation, especially when applied during high temperature processing, the lubricant should have a low degree of unsaturation, preferably less than about 15 as measured by iodine value. Examples of some suitable natural and synthetic ester lubricants include monoesters, diesters or polyesters such as pentaerythritol tetranonate, coconut oil, neopentyl glycol diisostearate, stearyl stearate. Examples of suitable natural and synthetic hydrocarbons are mineral oils and polyalphaolefins such as hydrogenated decene tetramer.

The finish composition also includes from about 1% to about 20% by weight of an alkali metal salt of a branched or unbranched aliphatic monocarboxylic acid containing at least 8 carbon atoms, preferably at least 14 carbon atoms. For convenience, the alkali metal salts of branched or unbranched aliphatic monocarboxylic acids having at least 8 carbon atoms will hereinafter be referred to as "soaps". Preferably, the composition comprises from about 2% to 15% % by weight of soap.

The soap may be a single soap; it may also be a mixture of soaps made, for example, of natural monocarboxylic acids or partly of natural monocarboxylic acids. The soap can also be a special blend for a particular finished use. Furthermore, in order to improve the performance against oxidative degradation, the above-mentioned soaps of branched or unbranched monocarboxylic acids should preferably contain not more than one carbon-carbon double bond.

It is necessary to use soaps in the composition which render the components liquid at temperatures below 150°C so that the composition is liquid at the temperature at which it is applied to the fibers. The temperature range for use of neat oily finishes is from 25°C to 150°C, preferably from 50°C to 100°C, therefore, it is preferred that the finish composition is liquid at temperatures below about 100°C. According to the present invention, soaps can be selected from a wide range, such as potassium stearate, potassium isostearate, sodium stearate, sodium isostearate and the like. However, certain soaps are difficult to use, especially depending on the alkali metal hydroxides used to prepare them, since such soaps may cause gelling of the composition. Soaps made from potassium salts or mixtures of potassium salts with other alkali metal hydroxides are preferred.

The soap in the finish acts as a surfactant and antistatic, thus eliminating static charges that build up on the yarn during fabrication and end-use handling.

The soap may be added to the finish or mixed with other finish combinations to obtain a finish composition, or preferably, the alkali metal hydroxide is added to a stirred mixture of one or more other finish agents at the point of use. Finishing agent ingredients, such as lubricants, nonionic surfactants (if any) and stabilizers (if any) are prepared from monocarboxylic acids. However, during in situ preparation, the amount of lubricant added should generally not be allowed to significantly exceed the amount of monocarboxylic acid added, because too much lubricant will interfere with proper mixing and will interfere with the addition of alkali metal salts. A solid was formed. All or the remainder of the lubricant should be added and mixed after soap preparation to form the finish composition.

For on-site preparation, the alkali metal salt should be dissolved in water to facilitate the neutralization reaction. However, the concentration of alkali metal hydroxide in the water should be high enough to ensure that the resulting finish does not contain too much water to cause phase separation to occur in the resulting finish. On the other hand, if a low concentration of alkali metal hydroxide is used, excess water can be removed after the neutralization reaction, thereby improving the uniformity of the finish. A suitable concentration of alkali metal hydroxide to avoid subsequent removal of water is in the range of 45-55% by weight. When two alkali metal hydroxides are used to form the soap, they can be added together or sequentially as desired.

The finishes of the present invention may be mixed with fully neutralized soaps or with soaps containing excess monocarboxylic acid or excess alkali metal hydroxide. For the vast majority of applications, it is believed to be preferable to use soaps with excess monocarboxylic acid in order to obtain uniformity of the finish and to avoid gelling of the finish, or to reduce irritation to meet occupational health concerns. relevant requirements. On the other hand, a slight excess of alkali metal hydroxide is also desirable in order to obtain the highest possible oxidation stability without causing phase separation effects or high viscosity problems. In the case of soap preparation in situ, the desired soap can be conveniently obtained by adjusting the ratio of monocarboxylic acid and alkali metal hydroxide.

Preferably, the finishes according to the invention are substantially free of nonionic surfactants. However, it is preferred that the finish composition contain no more than 5% by weight of nonionic surfactant for improved end use properties. Generally, to obtain any significant effect, the level of nonionic surfactant should be greater than 0.1%. Nonionic surfactants that can be used are ethoxylated carboxylic acids and ethoxylated alcohols. When sufficient nonionic surfactants are present, they may be suitable reaction media for making soaps in situ and require little or no addition of lubricant until soap is produced.

Preferably, for further thermo-oxidative stability, the finish composition includes from about 0.05% to about 5% by weight of a stabilizer. The stabilizer may be a single compound, such as an antioxidant, or a combination of stabilizers comprising an antioxidant together with additional materials for enhancing oxidative stability. Any of a wide variety of stabilizers known for finishing can be used in the finishing agent of the present invention as long as they can improve the performance of the finishing agent. A suitable stabilizer used according to the invention is, for example, a stabilizer component consisting of trilauryl phosphite and polydimethylsiloxane.

According to the present invention, the finish composition is intended to be applied to synthetic fibers as a neat oil, ie, when applied, the finish contains less than about 5% by weight of water. Preferably the finish is applied to a polymer selected from the class consisting of polyamide homopolymers and copolymers and polyester homopolymers and copolymers. While the finish has several beneficial uses, when the finish is applied to multiple yarns of as-spun fibers that are subsequently drawn (especially at high draw ratios and using high temperatures), When used, it is very suitable as a "spin finish". The finishes of the present invention may be applied by any of a number of known methods for applying pure oil-based finishes, such as using a rotating drum or metered tip dispenser. Preferably, the finish composition is applied at a temperature of about 25°C to 150°C, more preferably 50°C to 100°C. The preferred level of finish applied is about 0.2-2.0% by weight.

Test Methods:

Iodine value (AOCS method Cd 1-25) is determined by the Wijs method and is expressed as a percentage of iodine absorbed per gram of lubricant.

Viscosity was measured using a viscometer from Brookfield Engineering Laboratories, Inc., Stoughton, MA, USA, under the trademark BROOKFIELD(R) SYNCHKO-LECTRIC.

The pH is measured as a 5% by weight dispersion in demineralized water using a pH meter.

% Coating—film oven test Accurately weigh out 0.30-0.35 grams of finishing agent, put it into a pre-weighed, 57mm aluminum pan, and prepare for repeated experiments of several test finishing agents and standard finishing agents. These aluminum pans were randomly placed in 41cm x 23cm x 5cm (16″ x 19″ x 2″) enamel-coated steel pans, and it was placed in an electric pressure-ventilated oven. At a temperature of 225°C After 16 hours of exposure, remove the aluminum pan, let it cool at room temperature, and then re-measure the weight of the aluminum pan with the residue of the finishing agent. Then add 10-20 grams of acetone to the aluminum pan to remove the soluble After standing for 10 minutes, pour the acetone from the weighed aluminum pan, rinse with the acetone stream extruded from the plastic squeeze bottle, and clean up the residue that can be dissolved by acetone. Let the aluminum pan cool at 75°C Dry in an oven for about 10 minutes, then cool at room temperature, and finally measure the weight of the aluminum pan to calculate the percentage of the acetone-insoluble coating to the original sample weight.

Slurry Drain Test A solution consisting of 5 grams of polyacrylic acid reactive slurry and 95 grams of water was charged to a beaker with stirring and 3 grams of slip agent was added thereto. After 5 minutes had elapsed, stirring was stopped. After standing for one day, the finish is considered to have failed the slurry discharge test if a sticky film of the slurry had formed on the surface of the gum solution, or a sticky deposit had formed on the bottom of the slurry.

Example 1

Finishing agent samples A-D and comparison

The components and compositions of Finishing Samples A and B are shown in Table 1. The preparation method is to put all components except pentaerythritol tetranonate lubricant and potassium hydroxide (KOH) into a container , with mechanical stirring, a 45% aqueous solution of potassium oxyoxide was added on site to form a soap of potassium isostearate. After the addition, stirring was continued for another 10 minutes to ensure complete reaction, and then slowly while stirring Add pentaerythritol tetranonate lubricant to complete the preparation of pure oily finish.

The components and compositions of finishing agents C and D are shown in Table 1, and their preparation methods are similar to those described above. However, since these finishes do not contain nonionic surfactants, a portion of the pentaerythritol tetranonate lubricant (equal to the weight of isostearic acid) should be added in situ prior to the soap-forming neutralization step.

Several tests were carried out on the above-mentioned finishing agent in order to predict its performance in use, and the test results are listed in Table 2. The finishing agent used for reference is a pure oily finishing agent already used in commerce, and its composition is as follows:

69% coconut oil by weight;

30% by weight of sorbitol ethoxylate (nonionic surfactant);

1% by weight hindered phenol antioxidant

Example 2

Use finishing agent D to make a kind of 1260 denier (denier unit) as spinning finishing agent, its tenacity is the nylon 66 industrial yarn of 9.8gpd (per gram denier), and its process method is as U.S. Patent 3,311, No. 691 place stated. The finish was applied at about 80°C and was used in an amount of about 1.0% by weight. The spin performance observed was good, ie there were no adverse effects on spin breaks or broken filaments.

Table 1

  Finishing agent samples A B C D. Pentaerythritol tetrapelarganoate 89.16 88.16 90.86 91.96 Sorbitol/30EO/1 lauric acid/4 oleic acid 5.0 5.0 - - POE (14) isostearate - - 1.0 - Isostearic acid 5.0 5.0 7.0 7.0 Potassium hydroxide 0.3 0.3 0.5 0.5

(45% weight concentration) (0.67) (0.67) (1.11) (1.11) Sodium bis(2-ethylhexyl)sulfosuccinate - 1.0 0.1 - (75% weight concentration) - (1.33) (0.13) - Trilauric Phosphite 0.5 0.5 0.5 0.5 Polydimethylsiloxane (viscosity is 50cst) 0.04 0.04 0.04 0.04

Table 2

  Finishing agent samples A B C D Comparing Finishing Agents Viscosity@30℃pH@concentration 5%% coating 123456 average value slurry discharge test   48.09.300.790.631.020.620.790.360.70 failed 54.99.152.422.111.861.353.212.492.42 via 53.59.580.630.560.330.130.560.360.43 via 50.09.660.07-0.030.060.030.000.030.03 passed 71.06.0720.1418.6420.2117.8316.9618.8118.76 failed

Claims (19)

1. synthetic fiber with lubrication finishing agent composition coating, wherein said lubrication finishing agent composition comprises:

The lubricant of 80-99% weight, this lubricant are to be selected from by natural and synthesizing ester and to have number-average molecular weight to be at least 550amu, and its iodine number is lower than the class material that 15 natural and Synthin is formed; And

The monocarboxylic alkali metal salt of aliphatic of the side chain with at least 8 carbon atoms of 1-20% weight or non-side chain,

This finishing agent composition is a kind of liquid being lower than under 150 ℃ the temperature.

2. synthetic fiber according to claim 1, wherein said finishing agent composition comprises:

This lubricant of 85-98% weight; And

The monocarboxylic alkali metal salt of aliphatic of the side chain with at least 8 carbon atoms of 2-15% weight or non-side chain.

3. synthetic fiber according to claim 1, wherein the aliphatic unary carboxylation of side chain or non-side chain has at least 14 carbon atoms.

4. synthetic fiber according to claim 1, wherein this finishing agent composition contains the stabilizing agent of 0.05-5% weight.

5. synthetic fiber according to claim 1, wherein this finishing agent composition is substantially free of nonionic surface active agent.

6. synthetic fiber according to claim 1, wherein this fiber is the polymer of selecting in a kind of class material of being made up of polyamide homopolymer and copolymer and polyester homopolymer and copolymer.

7. synthetic fiber according to claim 1, wherein this finishing agent is to use on this fiber with the consumption of 0.2-2.0% weight.

8. one kind is coated on the lubrication finishing agent composition of synthetic fiber as pure finish, wherein comprises:

The lubricant of 80-99% weight, this lubricant are to be selected from by natural and synthesizing ester and to have number-average molecular weight to be at least 550amu, and its iodine number is lower than the class material that 15 natural and Synthin is formed; And

The monocarboxylic alkali metal salt of aliphatic of the side chain with at least 8 carbon atoms of 1-20% weight or non-side chain, wherein this alkali metal salt is to form by alkali metal hydroxide is added in the monocarboxylic acid at the scene,

This finishing agent composition is a kind of liquid being lower than under 150 ℃ the temperature.

9. finishing agent composition according to claim 8 wherein comprises:

This lubricant of 85-98% weight; And

The monocarboxylic alkali metal salt of aliphatic of the side chain with at least 8 carbon atoms of 2-15% weight or non-side chain.

10. finishing agent composition according to claim 8, wherein the aliphatic unary carboxylation of side chain or non-side chain has at least 14 carbon atoms.

11. finishing agent composition according to claim 8, wherein the aliphatic unary carboxylation of side chain or non-side chain is an isostearic acid potassium.

12. finishing agent composition according to claim 8 wherein comprises the stabilizing agent of 0.05-5% weight in addition.

13. finishing agent composition according to claim 8, wherein said composition is substantially free of nonionic surface active agent.

14. one kind is coated on the method for synthetic fiber with finishing agent, comprising in pure finish mode finishing agent composition as claimed in claim 8 being coated on these synthetic fiber.

15. method according to claim 14 when being coated onto this finishing agent composition on the fiber, is the temperature at 25 ℃ to 150 ℃ wherein.

16. method according to claim 14 when being coated onto this finishing agent composition on the fiber, is the temperature at 50 ℃ to 100 ℃ wherein.

17. method according to claim 14, wherein this finishing agent is that consumption with 0.2-2.0% weight is coated on this fiber.

18. method according to claim 14, wherein this fiber comprises a kind of polymer of selecting in the class material of being made up of polyamide homopolymer and copolymer and polyester homopolymer and copolymer.

19. method according to claim 14, wherein this fiber is a kind of as-spun fibre multiply yarn, and this yarn is stretched after coating this finishing agent composition.